CN101724388B - Cross-linking agent suitable for 160-200 DEG C stratum sand fracturing - Google Patents
Cross-linking agent suitable for 160-200 DEG C stratum sand fracturing Download PDFInfo
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- CN101724388B CN101724388B CN2009103112991A CN200910311299A CN101724388B CN 101724388 B CN101724388 B CN 101724388B CN 2009103112991 A CN2009103112991 A CN 2009103112991A CN 200910311299 A CN200910311299 A CN 200910311299A CN 101724388 B CN101724388 B CN 101724388B
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Abstract
The invention relates to a cross-linking agent which is suitable for 160-200 DEG C stratum sand fracturing. The cross-linking agent comprises a component A and a component B; the component A contains borate, zirconium compound and ligand, wherein the addition amount of the borate is 10-30 percent by weight, the addition amount of the zirconium compound is 5-15 percent by weight, the ligand is a mixture containing lactic acid, alkylol amine and acetic acid with the addition amount respectively of 2-5 percent, 4-9 percent and 1-2 percent by weight, and the balance is water; the component B is 10-30 percent of sodium hydroxide aqueous solution by weight; and the mixing weight ratio of the component A to the component B is 10: 1. The cross-linking agent has favorable cross-linking retardant performance and wider cross-linking ratio range; a water-base gel fracturing fluid formed by the cross-linking agent and a vegetable glue thickening agent has favorable thermal shear stability and high-speed viscosity recovery characteristic after shearing; and the residual content after gelout has low damage to a rock core.
Description
Technical field
The invention belongs to the oil-gas field development field, relate to a kind of oil-gas field high-temperature stratum fracturing liquid linking agent.
Background technology
Oil-gas field generally adopts fracturing technique to improve output at present, and along with the development of drilling and production technology, oil gas well newly developed often all is a deep layer, and high-temperature stratum is so have higher requirement to of the fracturing fluid temperature tolerance.Desire improves of the fracturing fluid temperature tolerance, need improve the each component performance in the fracturing liquid system, particularly the performance of linking agent.The common organic boron fracturing liquid linking agent that uses can only be applicable to that temperature is less than 150 ℃ of stratum at present, the crosslinked water-base gel fracturing fluid heat resistance of organic zirconium and organic titanium can reach 180 ℃, but the crosslinked fracturing fluid residue content of organic titanium and organic zirconium is very high, cause the injury of core very seriously, influenced post-fracturing correctional effect.
So at the oil gas well more than 160 ℃, need exploitation energy is high temperature resistant and core is injured little fracturing liquid at bottom temperature.And reach this purpose, developing high temperature resistant and eco-friendly linking agent is the task of top priority.
Summary of the invention
The object of the present invention is to provide a kind ofly to the low injury of stratum core, can be used for the linking agent of the sandfrac on 160 ℃ of-200 ℃ of stratum.
For achieving the above object, the invention provides following technical scheme.
Be applicable to the linking agent of 160 ℃ of-200 ℃ of stratum sand fracturings, by A, two kinds of components of B are formed, and the A component is generated under certain reaction conditions by borate, zirconium thing and part; The B component is the aqueous sodium hydroxide solution of 10-30 weight %.The weight ratio of A component and B component is 10: 1.
Borate in the described linking agent A component is ten water Sodium Tetraboratees, and dosage is 10-30 weight %, and best dosage is 15-22 weight %; The zirconium thing is the mixture of zirconium tetrachloride, zirconium dioxide or zirconium tetrachloride and zirconium dioxide, and dosage is 5-15 weight %; Part is lactic acid, hydramine, acetic acid, and dosage is respectively 2-5 weight %, 4-9 weight %, and 1-2 weight %, described hydramine can be Monoethanolamine MEA BASFs, diethanolamine or trolamine; All the other components are water.
The preparation process of linking agent of the present invention is as follows:
A component: in filling the 250ml three-necked flask bottle of water, add 10-30 weight % borate, 5-15 weight % zirconium thing, 80 ℃ were stirred 0.5-1 hour, the acetic acid of the lactic acid of adding 2-5 weight %, 4-9 weight % hydramine, 1-2 weight %, and 80 ℃ were stirred 6 hours.
The crosslinking agent B component mainly plays a part to regulate crosslinking time, and preparation process is as follows: in the 250ml flask, adding weight ratio is 10-30% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
Linking agent A, B component separated deposit, with linking agent A component and the B component weight ratio mixing for standby use with 10: 1, mixed use per-cent is 0.6 weight % during use.
Compared with prior art, this linking agent has the crosslinked scope that compares of good delayed cross-linking performance and broad, the water-base gel fracturing fluid that this linking agent and vegetable jelly viscosifying agent form has viscosity recovery feature after good thermal shear stability, the high speed shear, and residue content is low to the injury of core behind the broken glue.
Description of drawings
Fig. 1 is the flow curve of 198 ℃ of crosslinked gels;
Fig. 2 is the flow curve of 160 ℃ of crosslinked gels.
Embodiment
The preparation of linking agent
Embodiment 1
The preparation of A component: in the 250ml three-necked flask, add 20ml water, 10g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, add the 5g zirconium tetrachloride, 2g lactic acid, 4g trolamine, 1g acetic acid, add the water into 58ml, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 20% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 2
The preparation of A component: in the 250ml three-necked flask, add 39ml water, 30g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, adds the 15g zirconium tetrachloride, 5g lactic acid, the 9g trolamine, 2g acetic acid, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 20% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 3
The preparation of A component: in filling the 250ml three-necked flask of 30ml water, add 20g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, adds the 10g zirconium tetrachloride, 4g lactic acid, 7g trolamine, 2g acetic acid, add the water into 27ml, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 30% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 4
The preparation of A component: in filling the 250ml three-necked flask of 30ml water, add 20g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, adds the 10g zirconium dioxide, 4g lactic acid, 7g trolamine, 2g acetic acid, add the water into 27ml, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 10% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 5
The preparation of A component: in filling the 250ml three-necked flask of 30ml water, add 20g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, adds the 10g zirconium tetrachloride, 4g lactic acid, 6g diethanolamine, 2g acetic acid, add the water into 28ml, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 20% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 6
The preparation of A component: in filling the 250ml three-necked flask of 30ml water, add 20g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, adds the 10g zirconium tetrachloride, 4g lactic acid, 5g Monoethanolamine MEA BASF, 2g acetic acid, add the water into 29ml, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 20% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
Embodiment 7
The preparation of A component: in filling the 250ml three-necked flask of 44ml water, add 20g ten water Sodium Tetraboratees, stirring and refluxing is 1 hour in 80 ℃ of oil baths, add the 10g zirconium dioxide, 4g lactic acid, 6g diethanolamine, 2g acetic acid, 80 ℃ of stirring and refluxing 6 hours obtain weak yellow liquid.
The preparation of B component: in the 250ml flask, the adding weight ratio is 20% sodium hydroxide, adds entry and stirs, and dissolves fully up to sodium hydroxide.
A component and B component are mixed with 10: 1 weight ratio, promptly get linking agent.
The performance of linking agent
Embodiment 8
See Fig. 1.According to the base fluid of the method preparing fracturing fluid of patent (publication number CN1613957A), concrete compound method is as follows: thickening material 0.62%, tensio-active agent 0.123%, clay stabilizer 0.42%, sterilant 0.10%, buffer reagent 0.156%, temperature stabilising agent 0.27%.Add 0.6% linking agent that makes according to embodiment 3 in the fracturing liquid for preparing, fracturing liquid can become frozen glue in 10 minutes, become hanging property of frozen glue good.On the RS600 rheometer, test, under 198 ℃ of conditions, 170s
-1Viscosity remains on about 50-60mPa.s after shearing 30min continuously, and viscosity has by a relatively large margin after shear time extends to 60min, and viscosity rises to 60-90mPa.s behind the shearing 60-80min; Shear 120min, viscosity can remain on about 100mPa.s basically.
Embodiment 9
See Fig. 2.According to the base fluid of the method preparing fracturing fluid of embodiment 8, add 0.6% linking agent that makes according to embodiment 3 in the base fluid, fracturing liquid can become frozen glue in 10 minutes, become hanging property of frozen glue good.160 ℃, 170s
-1The high temperature evaluation result shows that this fracturing fluid gel viscosity remains on more than the 400mPa.s in 40min, viscosity remains on about 350mPa.s behind the shearing 60min; Its viscosity still remains on more than the 250mPa.s behind continuous shearing 120min.
Embodiment 10
Get frozen glue 1000ml, add the 300ppm ammonium persulphate, make its broken glue under 180 ℃ of conditions according to embodiment 8 preparations.Determine under the simulation downhole condition that with the core flow test broken fracturing fluid is to the injury situation on stratum, behind the crosslinked broken glue of frozen glue of linking agent of the present invention to the injury rate of core at 18-22%.
Claims (4)
1. be applicable to the linking agent of 160 ℃ of-200 ℃ of stratum sand fracturings, by A, two kinds of components of B are formed, A component preparation process is as follows: in filling the three-necked flask of water, add 10-30 weight % borate, 5-15 weight % zirconium thing, described zirconium thing is the mixture of zirconium tetrachloride, zirconium dioxide or zirconium tetrachloride and zirconium dioxide, and 80 ℃ were stirred 0.5-1 hour, add the lactic acid of 2-5 weight %, the hydramine of 4-9 weight %, the acetic acid of 1-2 weight %, 80 ℃ were stirred 6 hours; The B component is the aqueous sodium hydroxide solution of 10-30 weight %; A component and B component blended weight ratio are 10: 1.
2. linking agent as claimed in claim 1 is characterized in that, the borate in the described A component is ten water Sodium Tetraboratees.
3. linking agent as claimed in claim 1 is characterized in that, the borate dosage in the described A component is 15-22 weight %.
4. linking agent as claimed in claim 1 is characterized in that, the hydramine in the described A component part is Monoethanolamine MEA BASF, diethanolamine or trolamine.
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| CN101724388B true CN101724388B (en) | 2011-03-16 |
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Cited By (1)
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| CN105018066A (en) * | 2015-07-09 | 2015-11-04 | 陕西森瑞石油技术开发有限公司 | Crosslinking agent suitable for linear gel fracturing fluid, and preparation method thereof |
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| CN102212357A (en) * | 2010-04-09 | 2011-10-12 | 新疆荣森农业科技有限公司 | Preparation and application of water-based fracturing fluid organic zirconium high-temperature stabilizing agent for oil production |
| CN102040995B (en) * | 2010-11-11 | 2012-11-07 | 陕西科技大学 | Preparation method for high-temperature delay type organic zirconium cross-linking agent |
| CN102352231A (en) * | 2011-08-03 | 2012-02-15 | 西安长庆化工集团有限公司 | Hydrophobic modified hydroxypropyl guar fracturing liquid cross-linking agent and preparation method thereof |
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| CN103497753B (en) * | 2013-09-30 | 2016-01-20 | 西南石油大学 | One is applicable to the of the fracturing fluid linking agent of concentrated water |
| CN103881694B (en) * | 2014-03-20 | 2016-11-16 | 陕西省石油化工研究设计院 | A kind of low consumption guar gum multinuclear cross-linking agent |
| CN106318367A (en) * | 2016-08-17 | 2017-01-11 | 富象油气技术服务有限公司 | Ultrahigh temperature fracturing solution organic borate-zirconate crosslinking agent and preparation method thereof |
| US10669472B2 (en) * | 2017-03-01 | 2020-06-02 | Saudi Arabian Oil Company | Additives to minimize viscosity reduction for guar/borate system under high pressure |
| CN108485636B (en) * | 2018-04-16 | 2019-09-17 | 西南石油大学 | A kind of nanometer zirconium borate crosslinker resistant to high temperature and preparation method thereof |
| CN116120911A (en) * | 2023-01-09 | 2023-05-16 | 天津初心莫移科技有限责任公司 | Cross-linking agent emulsion for seawater-based fracturing fluid and preparation method thereof |
| CN116083069B (en) * | 2023-02-27 | 2024-05-17 | 中海油田服务股份有限公司 | Cross-linking agent for seawater-based fracturing fluid and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018066A (en) * | 2015-07-09 | 2015-11-04 | 陕西森瑞石油技术开发有限公司 | Crosslinking agent suitable for linear gel fracturing fluid, and preparation method thereof |
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